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Auto flammability

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Endpoint:
relative self-ignition temperature (solids)
Type of information:
experimental study
Adequacy of study:
key study
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
According to Directive 92/69/EEC and GLP
Qualifier:
according to guideline
Guideline:
EU Method A.16 (Relative Self-Ignition Temperature for Solids)
Version / remarks:
92/69/EEC, annex V, A.16.
GLP compliance:
yes
Key result
Relative self-ignition temperature:
>= 180 °C
Relative self-ignition temperature:
>= 340 °C

2 self-heating processes were recorded. The first one started at an onset temperature of 180°c and the second one started at 340°C with a maximum peak temperature of 510°C.

At the end of the measurment ash was remained in the wire basket.

Conclusions:
Due to the results from the A.16. test further studies are necessary to exclude or classify the substance as self-heating substance according to Regulation (EC) No 1272/2008.
Endpoint:
relative self-ignition temperature (solids)
Type of information:
experimental study
Adequacy of study:
key study
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
test procedure in accordance with national standard methods
Remarks:
according to Directive VDI 2263, part 1 (screening test) and according to DIN EN 15188 (main study)
Qualifier:
according to guideline
Guideline:
other: Directive VDI 2263, part 1
Version / remarks:
screening test
Qualifier:
according to guideline
Guideline:
DIN EN 15188 (Determination of the spontaneous ignition behaviour of dust accumulations)
GLP compliance:
no
Relative self-ignition temperature:
>= 150 °C
Remarks on result:
preliminary test
Remarks:
Grewer oven, result refers to the pure test material
Relative self-ignition temperature:
>= 180 °C
Remarks on result:
preliminary test
Remarks:
Grewer oven, result refers to the 1:1 kieselgur mixture
Relative self-ignition temperature:
>= 110 °C
Remarks on result:
other:
Remarks:
calculated result refers to 100 mm sample cube
Key result
Relative self-ignition temperature:
>= 135 °C
Remarks on result:
other:
Remarks:
calculated result refers to 25 mm sample cube

In the investigation of self-ignition in the Grewer oven for the pure test item an exothermic effect was observed starting at an onset temperature of 150 °C that led to a maximum temperature of approx. 440 °C. The same maximum temperature was recorded for the kieselgur mixture sample.

Isoperibolic hot storage experiment according to DIN EN 15188:

the sample was first heated to a storage temperature of 100°C. No self-heating was observed within 48 hours. Then the test item was heated with a heating rate of 1K/h, self-heating was recorded at an onset temperature of 108°C leading to a maximum temperature of > 500°C. After the test the sample was burnt.

Based on kinetic parameters and other relevant physical values determined in the study the self-heating temperature for classification-relevant sample volumes is calculated according to the theory of Frank-Kamenetskii:

- cubic mesh wire basket volume 1 L (edge length 100 mm): 110°C.

- cubic mesh wire basket volume 15.625 mL (edge length 25 mm): 135°C.

Conclusions:
According to the classification criteria of regulation (EC) 1272/2008 the test substance has to be classified as self-heating substance, category 1.
Executive summary:

The auto flammability of the test item was investigated first in a screening test according to Directive VDI 2263, part 1 (Grewer oven test). Self-heating was observed at an onset temperature of 150°C. As a consequence of this result an isoperibolic hot storage test according to DIN EN 15188 was conducted. In a 400 mL mesh wire basket self-heating was recorded at an onset temperature of 108°C.

The self-heating in different cubic mesh wire baskets (volumes 1 L and 15.625 mL) was calclulated based on the theory of Frank-Kamentskii using determined kinetic parameters, and other physical values like activation energy and thermal conductivity. The following results, self-heating below 140°C, were calculated:

- cubic mesh wire basket volume 1 L (edge length 10 cm): 110°C.

- cubic mesh wire basket volume 15.625 mL (edge length 2.5 cm): 135°C.

Therefore, the test item has to be classified according to regulation (EC) 1272/2008 as self-heating substance, category 1

Description of key information

Screening tests according to Directive VDI 2263, part 1 (Grewer oven) were conducted with 2 different test materials (studies 2003 and 2019). Self-heating was recorded at onset temperatures of 180°C and 150°C respectively.

Further investigations were necessary to exclude or classify the substance as self-heating substance according to Regulation (EC) No 1272/2008.

An isoberibolic hot storage test with a 400 mL mesh wire basket was conducted according to DIN EN 14188. Self-heating was observed at an onset temperature of 108°C. Based on this result and the determined corresponding parameters the self-heating temperature for relevant test item volumes were calculated:

- 100 mm sample cube: 110°C

- 25 mm sample cube: 135°C

According to the classification scheme of regulation (EC) 1272/2008, 2.11.1, the test item has to be classified as self-heating substance, category 1.

Key value for chemical safety assessment

Autoflammability / Self-ignition temperature at 101 325 Pa:
135 °C

Additional information

value refers to the 25 mm sample cube